CN106381540B - A kind of negative ion powder dispersion liquid and preparation method thereof being used to prepare anion viscose fibre - Google Patents
A kind of negative ion powder dispersion liquid and preparation method thereof being used to prepare anion viscose fibre Download PDFInfo
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- CN106381540B CN106381540B CN201610788524.0A CN201610788524A CN106381540B CN 106381540 B CN106381540 B CN 106381540B CN 201610788524 A CN201610788524 A CN 201610788524A CN 106381540 B CN106381540 B CN 106381540B
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- negative ion
- dispersant
- ion powder
- aqueous
- dispersion liquid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Abstract
The present invention relates to a kind of negative ion powder dispersion liquids and preparation method thereof being used to prepare anion viscose fibre, wherein the dispersion liquid includes negative ion powder, dispersant and electrolyte, it is dissolved in aqueous solution, wherein dispersant is first prepared into aqueous dispersant, and aqueous dispersant proportion is 1.35g/cm3~1.5g/cm3, the content in aqueous dispersant of dispersant is 2.5%~5%；The mass ratio of negative ion powder addition and dispersant addition be 5:1~10:1；The meltage of electrolyte is less than or equal to 0.3 μm in aqueous dispersant close to saturation or saturation, the middle grain size D50 of the negative ion powder dispersion liquid.It is 3%~6% that the negative ion powder dispersion liquid, which can be used for preparing with the high additive amount of negative ion powder, while fiber does fracture strength up to 2.2cN/dTex or more anion viscose fibres, and this method is easy to operate, economical, is suitable for industrialized production.
Description
Technical field
The present invention relates to weaving chemical field, particularly a kind of negative ion powders being used to prepare anion viscose fibre
Dispersion liquid and preparation method thereof.
Background technology
Viscose rayon belongs to staple fibre, is to be widely used a kind of general textile fabric at present, common viscose fiber tool
There are excellent wearability and extensive use scope.Viscose rayon forms alkali cellulose by native cellulose through alkalizing, then with
Carbon disulfide effect generates cellulose xanthate ester, is dissolved in the viscous solution obtained in dilute alkaline soln and claims viscose glue, viscose glue is through wet
After method spinning and a series for the treatment of process viscose rayon, the preparation process of common viscose fiber be known in the art.
With the improvement of people ' s living standards with the progress of textile industry technical merit, the various viscose glues with additional function
Fiber developed in succession, and especially the viscose rayon with negative ion releasing function is increasingly favored by people, right
Improve air quality, environment with apparent effect, there is good health-care effect to human body.
But in presently disclosed technology, the additional function in order to obtain viscose rayon is usually required in viscose rayon system
Specific additives is added during standby, can discharge anion mineral or other substances as being added, and the additives being added makes
Its intensity is lower, and addition is bigger, and intensity is lower, while may cause easily to reunite, settle, is unstable, so that spinning technique
Filtration difficulty etc..Lower tenacity fibers often make manufactured fabric that should not wash by rubbing with the hands strongly, and service life is short；Shrinkage height, washing
Appearance is undesirable afterwards；Poor flexibility, it is yielding etc..
The aqueous dispersion of negative ion powder is first made in the production method (CN1470684A) of viscose anion fiber, this method
Then liquid is added to before spinning in viscose rayon stoste, negative ion powder is added and accounts for the 1% of fiber total amount, increases one of mistake
Process is filtered, and optimizes spinning acid bath composition, the viscose rayon containing about 1% negative ion powder, the dry fracture of fiber has finally been made
Intensity is 1.88cN/dTex, wet breaking strength 0.99cN/dTex, dry elongation at break 17.4%.The preparation method subtracts
The additive amount of negative ion powder is lacked, while having enhanced stoste and filter and optimize coagulation bath composition and being improved spinnability.But it is fine
The additive amount for tieing up anion is on the low side and the physical property of fiber is made is declined, and the production cost of fiber also has by a relatively large margin
It improves.
It is viscous to disclose a kind of anion of textile manufacturing for anion viscose fibre and manufacturing method (1585565 A of CN)
Glue fiber and its manufacturing method, its main feature is that in fiber containing gross mass (8.6~9.2) % alpha cellulose, (5.35~
5.65) the ultra-fine granular tourmaline of the sodium hydroxide of %, (4~9) %.Manufacturing method is added containing above-mentioned before wet spinning
The functional finishing agent slurry of tourmaline, the average diameter containing (23~33) % is 0.65 μm in slurry tourmaline powder, (1~
2) % stearic acid (being mass ratio) and water.The dry fracture strength 2.02cN/dTex of the anion viscose fibre, wet fracture are strong
1.102cN/dTex is spent, dry elongation at break is 18.1%.The invention using stearic acid as tourmaline dispersion liquid made from dispersant,
Stability is poor, and stearic acid reacts to form sediment in viscose rayon spinning coagulation bath with divalent zinc ion, keeps coagulating bath transparent
Degree declines, and there may be spinning condition deterioration, coagulating bath filtration difficulties etc. therewith.
Therefore, a kind of can prepare with high-negative ion additive amount and the viscose rayon with high microsteping intensity, together is developed
When during viscose rayon stoste stablize, do not generate reunion, the preparation method of sedimentation is necessary, there is commercial Application meaning
Justice.
Invention content
Summary of the invention
The present inventor is attempted by test of many times, is developed one kind finally and can be prepared and has again with high-negative ion additive amount
There is the preparation method of the viscose rayon of high microsteping intensity.Thing is added into viscose rayon stoste before spinning in the preparation method
Then the anion dispersion liquid first prepared prepares, post-processing according to conventional spinning processes, then obtains viscose rayon.Wherein
The anion dispersion liquid includes negative ion powder, dispersant and electrolyte, is dissolved in the water.Usual negative ion powder dispersion liquid
In, because negative ion powder is than great, corase particles are easily precipitated and are reassociated, and the addition of the dispersant speed that makes to reassociate slows down；Electrolyte
Addition make the difference in specific gravity of negative ion powder and decentralized medium reduce, play the role of anti-settling agent.This method overcome high addition bear from
The common preparation problem encountered in sub- powder viscose rayon preparation process solves and prepares the easy reunion of additive viscose rayon, sinks
The problems such as shallow lake and viscose rayon stoste are unstable, this method is easy to operate, economical, is suitable for industrialized production.
First aspect present invention provides a kind of negative ion powder dispersion liquid being used to prepare anion viscose fibre.
Second aspect of the present invention provides a kind of preparation for the negative ion powder dispersion liquid being used to prepare anion viscose fibre
Method.
Third aspect present invention provides a kind of high-strength viscose glue anion viscose fibre of high additive amount.
Term defines
" water " means purified water or softened water in the present invention.
" % " unless otherwise stated, means mass percent in the present invention.
The density and the density under the pure water in standard atmospheric pressure, 3.98 DEG C that " proportion " means something in the present invention
The ratio of (999.972kg/m3).
It is meant in room temperature or 40 DEG C hereinafter, real-time when configuring dispersant solution " close to saturation or saturation " in the present invention
At a temperature of solute dissolved state.
" dry elongation at break (%) " refers to the ratio of elongate fiber degree and fiber raw footage when fiber does fracture in the present invention
Value, is length unit ratio.
Detailed description of the invention
First aspect present invention is intended to provide a kind of negative ion powder dispersion liquid being used to prepare anion viscose fibre, including
Negative ion powder, dispersant and electrolyte, are dissolved in aqueous solution；
It is prepared by the following method：
A) dispersant is dissolved completely in aqueous solution, electrolyte is then added, dissolving is complete, stirs evenly and is disperseed
Agent aqueous solution；
B) by negative ion powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50≤0.3 μm,
Obtain negative ion powder dispersion liquid；
The mass ratio of wherein the negative ion powder addition and dispersant addition is 5:1~10:1；
Wherein the aqueous dispersant proportion is 1.35g/cm3~1.5g/cm3, dispersant is in aqueous dispersant
Content be 2.5%~5%；
The meltage of electrolyte described in wherein is in aqueous dispersant close to saturation or saturation.
Grain size≤0.3 μm of anion powder of the present invention；In some embodiments≤0.2 μm.It has been investigated that
When the grain size≤0.3 μm spinning of anion powder changes a number and finished product fault greatly declines, spinnability greatly improves, and is conducive to just
The orientation stretching of raw silk item, fibre strength reach unanimity with common viscose fiber, and under common viscose fiber spinning technique, fiber is strong
Degree is up to 2.2cN/dTex or more, under high wet modulus or half koplon spinning process condition, the dry fracture of fiber
Intensity is up to 2.8cN/dTex or more.
In negative ion powder dispersion liquid of the present invention, because negative ion powder is than great, corase particles are easily precipitated and are reassociated, point
The addition of the powder speed that makes to reassociate slows down；The addition of electrolyte makes the difference in specific gravity of negative ion powder and decentralized medium reduce, and plays
The effect of anti-settling agent.Thus dispersant and electrolyte can be such that grinding more successfully carries out.
Negative ion powder of the present invention can be adapted for the minerals that can discharge anion applied in textile industry
Or the micro mist of other materials, including but not limited to tourmaline powder；
Dispersant of the present invention can be calgon, peregal or combinations thereof；
Electrolyte of the present invention can be salt acid sodium-salt, sodium sulfate salt, nitric acid sodium salt or sodium ascorbyl phosphate etc., Ru Shishui
Sodium sulphate etc.；
In order to accelerate the grinding of negative ion powder, the negative ion powder in the negative ion powder dispersion liquid can also first pass through alkali in advance
Solution impregnates, and structure dies down between making the crystal of negative ion powder, and wet lapping effect is made substantially to increase, and milling time shortens 3~4 times.
Aqueous slkali of the present invention can be the alkaline matter water that can ionize out hydroxyl radical negative ion in aqueous solution
Solution, such as 30% sodium hydrate aqueous solution.
Can be tourmaline powder in some embodiment negative ion powders, the mass ratio of addition and dispersant addition is 5:
1~10:1.
Dispersant is peregal or peregal and calgon in some embodiments, and aqueous dispersant proportion is
1.35g/cm3~1.5g/cm3, content of the dispersant in aqueous dispersant is 2.5%~5%.
Electrolyte can be sal glauberi in some embodiments, and the solubility in dispersion liquid is in saturation state
Or close saturation.
In some embodiments, negative ion powder is soaked in 30% sodium hydroxide in advance in room temperature or 40 DEG C of following temperature
Aqueous solution in, soaking time at least 12h or more or for 24 hours more than；In some embodiments, negative ion powder and 30% sodium hydroxide
Aqueous solution mass ratio >=1：4 or 1：5；It is filtered dry, cake moisture obtained is no more than 25% or 30%.
In some embodiments, the negative ion powder dispersion liquid of the present invention for being used to prepare anion viscose fibre, packet
Tourmaline powder, peregal, calgon and sal glauberi are included, is dissolved in aqueous solution；
It is prepared by the following method：
A) peregal and calgon being dissolved completely in aqueous solution, sal glauberi is then added, dissolving is complete,
Stir evenly acquisition aqueous dispersant；
B) by tourmaline powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50≤0.3 μm,
Obtain negative ion powder dispersion liquid；
The mass ratio of wherein the tourmaline powder addition and dispersant addition is 6.7:1；
Wherein the aqueous dispersant proportion is 1.43g/cm3, content of the peregal in aqueous dispersant be
1.1%, content of the calgon in aqueous dispersant is 2.2%.
The meltage of electrolyte described in wherein is in aqueous dispersant close to saturation or saturation；
Wherein the tourmaline powder is soaked in the water-soluble of 30% sodium hydroxide in advance in room temperature or 40 DEG C of following temperature
In liquid, soaking time at least 12h or more or for 24 hours more than, then filtering obtain, tourmaline powder and 30% sodium hydrate aqueous solution are dense
Spend ratio >=1：4 or 1：5；It is filtered dry, filter cake moisture ratio obtained is not to be exceeded 25% or 30%.
In some embodiments, the negative ion powder dispersion liquid of the present invention for being used to prepare anion viscose fibre, packet
Tourmaline powder, peregal and sal glauberi are included, is dissolved in aqueous solution；
Wherein it is prepared by the following method：
A) peregal is dissolved completely in aqueous solution, sal glauberi is then added, dissolving is complete, stirs evenly acquisition
Aqueous dispersant；
B) by tourmaline powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50≤0.3 μm,
Obtain negative ion powder dispersion liquid；
The mass ratio of wherein the tourmaline powder addition and dispersant addition is 5:1；
Wherein the aqueous dispersant proportion is 1.46g/cm3, content of the peregal in aqueous dispersant be
4.4%；
The meltage of electrolyte described in wherein is in aqueous dispersant close to saturation or saturation；
Wherein the tourmaline powder is soaked in the water-soluble of 30% sodium hydroxide in advance in room temperature or 40 DEG C of following temperature
In liquid, soaking time at least for 24 hours more than, then filtering obtains, tourmaline powder and 30% sodium hydrate aqueous solution concentration ratio >=1：
5；It is filtered dry, filter cake moisture ratio obtained is not to be exceeded 25%.
Second aspect of the present invention is intended to provide a kind of system for the negative ion powder dispersion liquid being used to prepare anion viscose fibre
Preparation Method includes the following steps：
A) aqueous dispersant is prepared, then electrolyte is added into aqueous dispersant, mixing obtains aqueous dispersant；
B) by negative ion powder be added to walk it is poly- b) prepare aqueous dispersant, stir evenly, be ground to middle grain size D50≤
0.3μm。
In some embodiments, b) negative ion powder that is added in step be it is pre- first pass through aqueous slkali soaking, then filtering obtains
.
In the method for the invention, by aqueous slkali soaking negative ion powder, structure dies down between making the crystal of negative ion powder, makes
Wet lapping effect substantially increases, and milling time shortens 3~4 times.
In some embodiments, negative ion powder is in being soaked in 30% aqueous slkali, soaking time at least 12h or more or for 24 hours
More than.
In some embodiments, negative ion powder soaking temperature is in 40 degree Celsius or less or room temperature.
In some embodiments, negative ion powder and aqueous slkali mass ratio >=1：4 or 1：5；It is filtered dry, filter cake cumulative water-oil ratio obtained
Example is not to be exceeded 25% or 30%.
In some embodiments, the mass ratio of negative ion powder addition and dispersant addition is 5:1~10:1 or 5:1.
In some embodiments, b) the prepared proportion for obtaining aqueous dispersant is 1.35g/cm3~1.5g/cm3, point
Content of the powder in aqueous dispersant is 2.5%~5%.
In some embodiments, b) described in grinding be in using zirconium oxide bead as the vertical grinding machine of abrasive media into
Row is used in combination laser particle analyzer to detect grain size, detection method：The container that grinding bead is added is fixed on the experiment of " quick worker " high speed coating
It is ground in machine, the measurement of first time fineness is carried out after 1h, detect a fineness every 0.5h later, grain size D50 is ground in the middle
When being milled to≤0.3 μm, stop grinding.
In some embodiments, a kind of preparation method for the negative ion powder dispersion liquid being used to prepare anion viscose fibre,
Include the following steps：
A) at normal temperatures, by 100g tourmaline powders be soaked in 30% sodium hydrate aqueous solution at least for 24 hours more than, electrically
Mountain flour and 30% sodium hydrate aqueous solution concentration ratio >=1:5, it is filtered dry, filtering obtains the filter cake that moisture ratio is no more than 25%；
B) 20g peregals are dissolved in aqueous solution, dissolving is complete, adds 150g sal glauberis until dissolving is close full
Or saturation, the proportion of aqueous dispersant is adjusted to 1.46g/cm3；
C) filter cake a) obtained is added in aqueous dispersant b) prepared, is stirred evenly, feeding is with zirconium oxide bead
It in the vertical grinding machine of abrasive media, is ground through Multi-path circulation, detects grain size with laser particle analyzer therebetween, grain size D50 is ground in the middle
When being milled to≤0.3 μm, stop grinding.
Negative ion powder, aqueous slkali, dispersant and electrolyte described in this preparation method and aforementioned negative ion powder dispersion liquid
Described in negative ion powder, aqueous slkali, the explanation of dispersant and electrolyte it is consistent.
The above-described negative ion powder dispersion liquid of the present invention can be used for preparing anion viscose fibre, particularly suitable for
Prepare the high-strength viscose glue anion viscose fibre of high additive amount.It needs the series for discharging anion higher according to viscose rayon, needs
It is added that corresponding negative ion powder is more in viscose rayon, but more obtained viscose rayons are added in the additives such as negative ion powder
Intensity is lower, and the two is difficult to take into account, this is common sense in the field and technical problem.Using anion dispersion liquid of the present invention,
It is added in anion viscose fibre preparation process by corresponding method, negative ion powder additive amount may be implemented and reach 3%~6%
(mass ratio of negative ion powder dry weight and first kind fiber in viscose rayon), while the dry fracture strength of viscose rayon still exists
More than 2.2cN/dTex.
Here, the present invention provides a kind of high high-strength viscose glue anion viscose fibre of additive amount, it is characterized in that passing through following step
It is rapid to prepare：
A) the above-described any anion dispersion liquid of the present invention is added in the viscose rayon stoste before spinning；
B) and then anion viscose fibre is made in spinning, aftertreatment technology spinning；
Wherein the anion additive amount is 3%~6%, and negative ion powder dry weight is to alpha cellulose quality；Viscose glue is fine
Dimension does fracture strength up to 2.2cN/dTex or more.
Viscose rayon stoste can be passed through using native cellulose according to preparation method conventional in fibrous woven industry
The processes such as dipping, squeezing, crushing, aging, yellow, dissolving, maturation, filtering, deaeration prepare.
The method that anion viscose fibre is made in follow-up spinning, aftertreatment technology spinning, according to can be in common sense in the field
It is to use wet spinning, viscose glue forms thread by spinneret orifice and enters the coagulating bath containing acid, and alkali is neutralized in viscose glue, and thread is frozen into
Strand, cellulose xanthate disintegrating and regeneration is at cellulose hydrate；Then post-processing commonly used in the art is can be selectively performed,
Such as washing, pickling, oils and dries post-processing processing at desulfurization, to realize following process purpose.
In some embodiments, anion dispersion liquid of the present invention is added to the side in viscose rayon stoste before spinning
Method is before metering pump and quiet, dynamic mixer are added directly into spinning in a manner of being injected before spinning, equally with metering pump
In the viscose rayon stoste for measuring conveying.
Using injection device before spinning, anion dispersion liquid is injected into before spinning is spun in stoste, then spinning is compared it
It is added to after yellow before three (or four) filtering, until fibre solidification, the distance that anion particle is passed by is short, advantageously reduces
The possibility to reassociate.In addition, because of a large amount of electrolyte of content in anion dispersion liquid, position should not also add in stoste addition
Entered forward, and otherwise can lead to the fluctuation of viscose ripening degree, and influenced spinnability and finished fiber intensity to the greatest extent.
Negative ion powder dispersion liquid provided by the invention can be used for preparing anion viscose fibre, particularly suitable for preparing
The high high-strength viscose glue anion viscose fibre of additive amount, negative ion powder additive amount can reach 3% or more, and (negative ion powder dry weight is to first kind
Cellulose quality), while viscose rayon obtained does fracture strength up to 2.2cN/dTex or more.Technology provided by the invention
Scheme overcomes the technical difficulty for preparing the high high-strength viscose glue anion viscose fibre of additive amount, efficiently solves described in preparation
The easy reunion that is commonly encountered in fiber, the problems such as precipitation and viscose rayon stoste are unstable, make up defect in the prior art.
Negative ion powder additive amount provided by the invention is 3%~6% simultaneously, and negative ion powder dry weight is to alpha cellulose matter
Amount, while viscose rayon obtained is done fracture strength and is had very in fact up to the anion viscose fibre of 2.2cN/dTex or more
Value solves the demand of current textile industry and the high-strength negative-ion fiber of people, has significant progress.
Specific implementation mode
In order to make those skilled in the art more fully understand technical scheme of the present invention, it is non-that some are disclosed further below
Limiting embodiment, the present invention is described in further detail.
Reagent used in the present invention can be bought or can described method system through the invention from the market
It is standby and obtain.
Embodiment 1
Anion dispersion liquid and preparation：
| Component | Weight (g) |
| Tourmaline powder | 100 |
| Peregal | 20 |
| Sal glauberi | 150 |
Tourmaline powder 100g is weighed in 1L beakers, is added containing 30% sodium hydroxide 500g, is impregnated for 24 hours, Buchner funnel
Suction strainer is filtered dry, and is weighed as 139g.
Prepare aqueous dispersant：Claim peregal 20g, sal glauberi 150g, be added to after mixing in 1 liter of beaker, is delayed
Slowly add deionized water, be added while stirring, until solid mixture all dissolves, dispersant is weighed as 455g, surveys proportion and is
1.46g/cm3。
It by 139g filter cakes, is added in 455g aqueous dispersants, stirs evenly, in empirical formula vertical lapping machine, add
The zirconium oxide bead for entering a diameter of 2.0~2.8mm of 500g is ground, and is detected therebetween with laser particle analyzer, waits for middle grain size D50 grindings
When to 0.3 micron, stops grinding, filter out zirconium pearl；Negative ion powder dispersion liquid is spare.
It is prepared by anion viscose fibre：
It is straight in a manner of being injected before spinning metering pump and quiet, dynamic mixer by ground negative ion powder dispersion liquid
It connects in viscose rayon stoste before being added to spinning, equally to measure pump-metered conveying, anion additive amount is 5.5% (negative
Ion dried bean noodles is again to alpha cellulose quality), it is pumped into spinning coagulation bath through spinning measuring, then routinely spinning, post-processing
Anion viscose fibre is made in technique spinning.
Embodiment 2
Anion dispersion liquid and preparation：
| Component | Weight (g) |
| Tourmaline powder | 100 |
| Calgon | 10 |
| Peregal | 5 |
| Sal glauberi | 150 |
Tourmaline powder 100g is weighed in 1L beakers, is added containing 30% sodium hydroxide 500g, is impregnated for 24 hours, Buchner funnel
Suction strainer is filtered dry, and is weighed as 140g.
Prepare aqueous dispersant：Calgon 10g, peregal 5g, sal glauberi 150g is claimed to be added to after mixing
In 1 liter of beaker, slowly add deionized water, be added while stirring, until solid mixture all dissolves, dispersant is weighed as
450g, survey proportion are 1.43g/cm3。
It by 140g filter cakes, is added in 450g aqueous dispersants, stirs evenly, in empirical formula vertical lapping machine, add
The zirconium oxide bead for entering a diameter of 2.0~2.8mm of 500g is ground, and is detected therebetween with laser particle analyzer, waits for middle grain size D50 grindings
When to 0.3 micron, stops grinding, filter out zirconium pearl；Negative ion powder dispersion liquid is spare.
It is prepared by anion viscose fibre：
It is straight in a manner of being injected before spinning metering pump and quiet, dynamic mixer by ground negative ion powder dispersion liquid
It connects in viscose rayon stoste before being added to spinning, equally to measure pump-metered conveying, anion additive amount is 3.1% (negative
Ion dried bean noodles is again to alpha cellulose quality), it is pumped into spinning coagulation bath through spinning measuring, then routinely spinning, post-processing
Anion viscose fibre is made in technique spinning.
Embodiment 3
Anion dispersion liquid and preparation：
| Component | Weight (g) |
| Tourmaline powder | 100 |
| Peregal | 25 |
| Sal glauberi | 150 |
Tourmaline powder 100g is weighed in 1L beakers, is added containing 30% sodium hydroxide 500g, is impregnated for 24 hours, Buchner funnel
Suction strainer is filtered dry, and is weighed as 142g.
Prepare aqueous dispersant：Claim peregal 25g, sal glauberi 150g, be added to after mixing in 1 liter of beaker, is delayed
Slowly add deionized water, be added while stirring, until solid mixture all dissolves, dispersant is weighed as 460g, surveys proportion and is
1.49g/cm3。
It by 142g filter cakes, is added in 460g aqueous dispersants, stirs evenly, in empirical formula vertical lapping machine, add
The zirconium oxide bead for entering a diameter of 2.0~2.8mm of 500g is ground, and is detected therebetween with laser particle analyzer, waits for middle grain size D50 grindings
When to 0.3 micron, stops grinding, filter out zirconium pearl；Negative ion powder dispersion liquid is spare.
It is prepared by anion viscose fibre：
It is straight in a manner of being injected before spinning metering pump and quiet, dynamic mixer by ground negative ion powder dispersion liquid
It connects in viscose rayon stoste before being added to spinning, equally to measure pump-metered conveying, anion additive amount is 4.5% (negative
Ion dried bean noodles is again to alpha cellulose quality), it is pumped into spinning coagulation bath through spinning measuring, then routinely spinning, post-processing
Anion viscose fibre is made in technique spinning.
4 comparative example 1 of embodiment
Anion dispersion liquid and preparation：
| Component | Weight (g) |
| Tourmaline powder | 100 |
| Peregal | 5 |
| Sal glauberi | 150 |
Tourmaline powder 100g is weighed in 1L beakers, is added containing 30% sodium hydroxide 500g, impregnates 12h, Buchner funnel
Suction strainer is weighed as 155g.
Prepare aqueous dispersant：Claim peregal 5g, sal glauberi 150g, is added to after mixing in 1 liter of beaker, slowly
Add deionized water, be added while stirring, until solid mixture all dissolves, dispersant is weighed as 440g, surveys proportion and is
1.32g/cm3。
It by 155g filter cakes, is added in 440g aqueous dispersants, stirs evenly, in empirical formula vertical lapping machine, add
The zirconium oxide bead for entering a diameter of 2.0~2.8mm of 500g is ground, and is detected therebetween with laser particle analyzer, waits for middle grain size D50 grindings
When to 0.5 micron, stops grinding, filter out zirconium pearl；Negative ion powder dispersion liquid is spare.
It is prepared by anion viscose fibre：
It is straight in a manner of being injected before spinning metering pump and quiet, dynamic mixer by ground negative ion powder dispersion liquid
It connects in viscose rayon stoste before being added to spinning, equally to measure pump-metered conveying, anion additive amount is 4.0% (negative
Ion dried bean noodles is again to alpha cellulose quality), it is pumped into spinning coagulation bath through spinning measuring, then routinely spinning, post-processing
Anion viscose fibre is made in technique spinning.
Conglomerate causes to filter relative difficulty than more serious in viscose rayon spinning process.
5 comparative example 2 of embodiment
Anion dispersion liquid and preparation：
| Component | Weight (g) |
| Tourmaline powder | 100 |
| Peregal | 35 |
| Sal glauberi | 150 |
Tourmaline powder 100g is weighed in 1L beakers, is added containing 30% sodium hydroxide 500g, impregnates 12h, Buchner funnel
Suction strainer is weighed as 160g.
Prepare aqueous dispersant：Claim peregal 35g, sal glauberi 150g, be added to after mixing in 1 liter of beaker, is delayed
Slowly add deionized water, be added while stirring, until solid mixture all dissolves, dispersant is weighed as 465g, surveys proportion and is
1.55g/cm3。
It by 160g filter cakes, is added in 465g aqueous dispersants, stirs evenly, in empirical formula vertical lapping machine, add
The zirconium oxide bead for entering a diameter of 2.0~2.8mm of 500g is ground, and is detected therebetween with laser particle analyzer, waits for middle grain size D50 grindings
When to 0.5 micron, stops grinding, filter out zirconium pearl；Negative ion powder dispersion liquid is spare.
It is prepared by anion viscose fibre：
It is straight in a manner of being injected before spinning metering pump and quiet, dynamic mixer by ground negative ion powder dispersion liquid
It connects in viscose rayon stoste before being added to spinning, equally to measure pump-metered conveying, anion additive amount is 3.9% (negative
Ion dried bean noodles is again to alpha cellulose quality), it is pumped into spinning coagulation bath through spinning measuring, then routinely spinning, post-processing
Anion viscose fibre is made in technique spinning.
Embodiment 6
The unit area anion burst size for the anion viscose fibre that detection embodiment 1-5 is prepared respectively, fiber
The negative of different example schemes acquisitions is investigated in dry fracture strength, fiber wet breaking strength and the dry elongation at break of fiber, comparison
The relevant parameter of ion viscose rayon.
To sum up described in embodiment, anion viscose fibre that technical solution that embodiment 1-3 is provided prepares has negative
The high additive amount of ion powder has good anion release and good fibre strength.And the technology that embodiment 4 or 5 provides
Scheme, the anion dispersion liquid used are different from embodiment 1-3, for example, the water content of filter cake is bigger and embodiment 4
The content in aqueous dispersant of dispersant is 1.14%, the content in aqueous dispersant of 4 dispersant of embodiment
It is 7.50% etc., causes embodiment 4 or 5 to prepare anion viscose fibre performance undesirable.
Therefore, technical solution provided by the invention successfully solves technological deficiency existing for this field, successfully prepare bear from
Sub- powder additive amount is 3%~6%, and for negative ion powder dry weight to alpha cellulose quality, it is reachable that viscose rayon does fracture strength
The anion viscose fibre of 2.2cN/dTex or more has positive progressive.
The method of the present invention is described by preferred embodiment, related personnel can obviously hold within the present invention,
Method described herein and application are modified or are suitably changed and combined in spirit and scope, to realize and apply the present invention
Technology.Those skilled in the art can use for reference present disclosure, be suitably modified technological parameter realization.In particular, it should be pointed out that institute
There are similar replacement and change apparent to those skilled in the art, they are considered as being included in the present invention
It is interior.
Claims (8)
1. a kind of negative ion powder dispersion liquid being used to prepare anion viscose fibre, including negative ion powder, dispersant and electrolyte,
It is dissolved in aqueous solution；
It is prepared by the following method：
A) dispersant is dissolved completely in aqueous solution, electrolyte is then added, dissolving is complete, stirs evenly and obtains dispersant water
Solution；
B) by negative ion powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50 It≤0.3 μm, obtains
Negative ion powder dispersion liquid；
The mass ratio of wherein the negative ion powder addition and dispersant addition is 5:1~10:1；
Wherein the aqueous dispersant proportion is 1.35g/cm3~1.5g/cm3, dispersant containing in aqueous dispersant
Amount is 2.5%~5%；The meltage of electrolyte described in wherein is in aqueous dispersant close to saturation or saturation.
2. negative ion powder dispersion liquid according to claim 1, wherein the negative ion powder is pre- to first pass through aqueous slkali soaking
's.
3. negative ion powder dispersion liquid according to claim 2, negative ion powder in 40 DEG C of following temperature, are soaked in advance
In the aqueous solution of 30% sodium hydroxide, soaking time at least 12h or more；Negative ion powder and 30% sodium hydrate aqueous solution mass ratio
≥1：5；It is filtered dry, cake moisture obtained is no more than 30%.
4. a kind of negative ion powder dispersion liquid being used to prepare anion viscose fibre, including tourmaline powder, peregal, hexa metaphosphoric acid
Sodium and sal glauberi, are dissolved in aqueous solution；
It is prepared by the following method：
A) peregal and calgon are dissolved completely in aqueous solution, sal glauberi is then added, dissolving is complete, stirring
Uniformly obtain aqueous dispersant；
B) by tourmaline powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50 It≤0.3 μm, obtains
Negative ion powder dispersion liquid；
The mass ratio of wherein the tourmaline powder addition and dispersant addition is 6.7:1；
Wherein the aqueous dispersant proportion is 1.43g/cm3, content of the peregal in aqueous dispersant is 1.1%,
Content of the calgon in aqueous dispersant is 2.2%；
The meltage of sal glauberi described in wherein is in aqueous dispersant close to saturation or saturation；
Wherein the tourmaline powder is soaked in advance in 40 DEG C of following temperature in the aqueous solution of 30% sodium hydroxide, is impregnated
Time at least for 24 hours more than, then filtering obtains, tourmaline powder and 30% sodium hydrate aqueous solution concentration ratio >=1：5；It is filtered dry, makes
The filter cake moisture ratio obtained is not to be exceeded 30%.
5. a kind of negative ion powder dispersion liquid being used to prepare anion viscose fibre, including tourmaline powder, peregal and ten water sulphur
Sour sodium, is dissolved in aqueous solution；
Wherein it is prepared by the following method：
A) peregal is dissolved completely in aqueous solution, sal glauberi is then added, dissolving is complete, stirs evenly and is disperseed
Agent aqueous solution；
B) by tourmaline powder be added a) obtained by aqueous dispersant, stir evenly, be ground to middle grain size D50 It≤0.3 μm, obtains
Negative ion powder dispersion liquid；
The mass ratio of wherein the tourmaline powder addition and dispersant addition is 5:1；
Wherein the aqueous dispersant proportion is 1.46g/cm3, content of the peregal in aqueous dispersant is 4.4%；
The meltage of sal glauberi described in wherein is in aqueous dispersant close to saturation or saturation；
Wherein the tourmaline powder is soaked in the aqueous solution of 30% sodium hydroxide, soaking time is at least in advance in room temperature
More than for 24 hours, then filtering obtains, tourmaline powder and 30% sodium hydrate aqueous solution concentration ratio >=1：5；It is filtered dry, filter cake obtained
Moisture ratio is not to be exceeded 25%.
6. a kind of method of the negative ion powder dispersion liquid prepared described in claim 5 comprising following steps：
A) at normal temperatures, by 100g tourmaline powders be soaked in 30% sodium hydrate aqueous solution at least for 24 hours more than, tourmaline powder
With 30% sodium hydrate aqueous solution concentration ratio >=1:5, it is filtered dry, filtering obtains the filter cake that moisture ratio is no more than 25%；
B) 20g peregals are dissolved in aqueous solution, dissolving is complete, adds 150g sal glauberis until dissolving is close full or full
With adjust the proportion of aqueous dispersant to 1.46g/cm3；
C) filter cake a) obtained is added in aqueous dispersant b) prepared, is stirred evenly, it is grinding to be sent into zirconium oxide bead
It in the vertical grinding machine of medium, is ground through Multi-path circulation, detects grain size with laser particle analyzer therebetween, in the middle grain size D50Be ground to≤
At 0.3 μm, stop grinding.
7. a kind of anion viscose fibre is obtained by following preparation method：
A) any anion dispersion liquids of claim 1-5 is used to be added in the viscose rayon stoste before spinning；
B) and then anion viscose fibre is made in spinning, aftertreatment technology spinning；
Wherein, negative ion powder additive amount is 3%~6%, and negative ion powder dry weight is to alpha cellulose quality.
8. anion viscose fibre according to claim 7, intermediate ion dispersion liquid is added to the viscose rayon before spinning
Stoste is same with metering pump before metering pump and quiet, dynamic mixer are added directly into spinning in a manner of being injected before spinning
In the viscose rayon stoste for measuring conveying.
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| CN109321991A (en) * | 2018-11-09 | 2019-02-12 | 山东欣悦健康科技有限公司 | A kind of multi-functional composite additive, with antibacterial, anti-mite, the viscose rayon of hair tonic anion function and preparation method thereof |
| CN112044295A (en) * | 2020-08-19 | 2020-12-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Nano tourmaline dispersion liquid and preparation method thereof |
| CN113718361A (en) * | 2021-09-18 | 2021-11-30 | 南通强生石墨烯科技有限公司 | Graphene anion regenerated cellulose composite fiber and preparation method thereof |
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| US4325741A (en) * | 1979-09-20 | 1982-04-20 | Kanebo, Ltd. | Fibroin-coated pigment and processes for producing same |
| CN1470684A (en) * | 2002-07-22 | 2004-01-28 | 新乡化纤股份有限公司 | Method for producing glued negative ion fiber |
| CN1958894A (en) * | 2005-11-06 | 2007-05-09 | 杨秀珍 | Negative ion polyacrylonitrile fiber of releasing negative ion, and containing not radiant material |
| CN102121139A (en) * | 2011-01-11 | 2011-07-13 | 上海珍奥生物科技有限公司 | Preparation method of tourmaline viscose fibers |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4325741A (en) * | 1979-09-20 | 1982-04-20 | Kanebo, Ltd. | Fibroin-coated pigment and processes for producing same |
| CN1470684A (en) * | 2002-07-22 | 2004-01-28 | 新乡化纤股份有限公司 | Method for producing glued negative ion fiber |
| CN1958894A (en) * | 2005-11-06 | 2007-05-09 | 杨秀珍 | Negative ion polyacrylonitrile fiber of releasing negative ion, and containing not radiant material |
| CN102121139A (en) * | 2011-01-11 | 2011-07-13 | 上海珍奥生物科技有限公司 | Preparation method of tourmaline viscose fibers |
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